CN102272891A - Internally modified substrate for epitaxial growth, crystal film-forming body, device, bulk substrate manufactured using same, and their manufacturing method - Google Patents
Internally modified substrate for epitaxial growth, crystal film-forming body, device, bulk substrate manufactured using same, and their manufacturing method Download PDFInfo
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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Abstract
Provided is a sapphire substrate mainly for epitaxial growth of a nitride semiconductor layer, wherein the shape and/or the amount of deflection of the substrate can be efficiently and accurately controlled; and the deflection of the substrate occurring when a film is formed is suppressed so that the deflection behavior of the substrate can be reduced. Further, a film forming element for a nitride semiconductor layer, a nitride semiconductor device, and a nitride semiconductor bulk substrate, which are produced using the sapphire substrate, and a method for producing the same are provided. Pulse lasers are concentrated in the inside of the sapphire substrate through the polished surface of the sapphire substrate, to scan the inside of the sapphire substrate, and reforming region patterns are formed using multiphoton absorption performed by the pulse lasers, so that the shape and/or the amount of deflection of the substrate can be controlled. When a nitride semiconductor layer is formed using the sapphire substrate, the deflection of the substrate occurring when a film is formed can be suppressed, and the deflection behavior of the substrate can be reduced. Thus, the quality and the uniformity of the film can be improved, and the quality and the yield ratio of the nitride semiconductor device can be improved.
Description
Technical field
What the present invention relates to is crystal phragmoplast, device, bulk substrate and their manufacture method of epitaxial growth with inter-modification substrate and its manufacturing of use.
Background technology
With the gallium nitride is the nitride-based semiconductor of representative, because band gap is wide and can to send blueness be light, therefore, is widely used in LED (light-emitting diode) or LD (semiconductor laser) etc.In recent years, the research of further raising luminous efficiency or high brightnessization is carried out widely.
General nitride semiconductor luminescent element structure, the double-heterostructure of the n type covering that has on Sapphire Substrate n type contact layer that lamination successively has the resilient coating that is made of GaN, is made of n type GaN, constitutes by n type AlGaN, the active layer that constitutes by n type InGaN, the p type covering that constitutes by p type AlGaN, the p type contact layer that constitutes by p type GaN.Active layer constitutes only to comprise and has by In
xGa
L-xSingle quantum well (the SQW:Single Quantum Well) structure of the trap layer that N (0≤X≤1) constitutes or by In
xGa
1-xThe trap layer that N (0≤X≤1) constitutes and by In
yGa
1-yN (the In (patent documentation 1) in Multiple Quantum Well (the MQW:Multi Quantum Well) structure on the barrier layer of 0≤y≤1, y＜x) constitute.
When on Sapphire Substrate, making above-mentioned gallium nitride layer epitaxial growth, result from gallium nitride and sapphire coefficient of thermal expansion differences and lattice constant difference and on the Sapphire Substrate after the film forming, produce the situation of warpage, by cognition.
In non-patent literature 1, to epitaxial growth AlN resilient coating on Sapphire Substrate and GaN layer and how relax the thermal stress that produces by film forming, investigate according to the film thickness of GaN layer.In this non-patent literature 1, the warpage of substrate becomes big along with the film thickness thickening, produce the situation that boundary defect (Interface Defects), microfissure (Microcracks) or dislocation (Dislocation), macroscopic cracking (Macrocracks) relax stress by following, by clearly in this.
In addition, in Fig. 4 of non-patent literature 2, disclose being that the warpage of the substrate that produces of the operation of LED structure is carried out the analytical method that In-situ (original position) observes by epitaxial growth GaN on Sapphire Substrate.By like this, find in a series of film formation process, owing to the variation of film forming matter, film-forming temperature, film thickness significantly changes the curvature of Sapphire Substrate.
And, be almost 0 such film formation process by the curvature that is formed on as Sapphire Substrate in the growth phase of the InGaN layer of active layer, and make the situation of the emission wavelength homogenizing in the substrate surface, also by clearly.
As mentioned above, the warpage by a series of film formation process Sapphire Substrate significantly changes as can be known, thereby the quality of nitride semiconductor film or the uniformity of emission wavelength are brought influence.
In fact, utilizing the coefficient of thermal expansion differences with substrate, is that substrate curvature is almost 0 like that in the active layer with InGaN, and sets the warped shapes and the amount of warpage of Sapphire Substrate.Under such background,, and various grinding technology (for example patent documentation 2) have been studied for shape and the amount of warpage of controlling Sapphire Substrate.
On the other hand, when the light-emitting component that the Sapphire Substrate upper strata is pressed with nitride-based semiconductor is cut apart, in the inside of Sapphire Substrate, assemble pulse laser and form the technology of cutting apart the corresponding modification area of preset lines with light-emitting component by cognitive (patent documentation 3) with the thickness about 80～90 μ m.The invention of patent documentation 3 even be that Sapphire Substrate irradiating laser light is divided into each light-emitting component, also can suppress the processing method of the Sapphire Substrate that the brightness of light-emitting component reduces, with the purpose that is divided into of light-emitting component.
Patent documentation 1: No. the 3250438th, day disclosure communique, special permission
Patent documentation 2: day disclosure communique, spy open 2006-347776 number
Patent documentation 3: day disclosure communique, spy open 2008-6492 number
Non-patent literature 1:Jpn.J.Appl.Phys.Vol.32 (1993) pp.1528-1533
Non-patent literature 2:J.Cryst.Growth, Vol.272, lssues 1-4, (2004), pp.94-99
Summary of the invention
As mentioned above, exist owing to the warpage of Sapphire Substrate is significantly changed by a series of film formation process that obtain LED structure with gallium nitride system, thereby the uniformity variation of the quality of nitride semiconductor layer or emission wavelength, thereby the such problem of rate of finished products step-down of light-emitting diode.
At this problem, in existing method, adopt so that InGaN is the curvature of the substrate in the growth phase of active layer is almost 0 and sets the warped shapes of Sapphire Substrate and the method for amount of warpage like that.Just, in advance Sapphire Substrate being given at InGaN is that the amount of warpage that produces in the growth phase of active layer is partly offset such method.By like this, though can suppress the deviation of emission wavelength to a certain degree,, the problem that exists in InGaN and be the warpage of the substrate that produces in the film forming engineering beyond the active layer can't solve such problem.
Particularly, when n-GaN layer growth stage or film forming finish back cooling substrate, because Sapphire Substrate warpage significantly, therefore exist film quality and film quality uniformity to reduce or problem that the brilliant back-grinding processing of substrate can't be carried out etc. equably.Because these problems significantly influence the rate of finished products of devices such as light-emitting diode, therefore, need suppress the warpage and the variable quantity thereof of substrate by film formation process integral body, thereby reduce the buckling behavior of substrate itself, still, such Sapphire Substrate does not exist at present.
In addition, when making the Sapphire Substrate heavy caliber, exist the warped shapes utilize the precision that attrition process carries out and the control of amount of warpage itself to become difficult such problem.In the Sapphire Substrate of having implemented attrition process, usually because the difference of the accurately machined surface roughness of the residual or top and bottom of machining deformation and on substrate, produce the situation of warpage, by cognition.For example, in the polished substrate of single face, mainly be the main cause that the surface roughness difference of top and bottom becomes warpage, in two-sided polished substrate, except the surface roughness of top and bottom was slightly different, the surface roughness in substrate surface deviation slightly also became the main cause of warpage.
Particularly, in the heavy caliber substrate, making surface roughness in the substrate surface become evenly is difficult technically, thereby only has the problem that can't critically be controlled to the such technical limitations of desirable warped shapes and amount of warpage by attrition process.
In addition, if obtain the nitride-based semiconductor bulk substrate, and the thick film epitaxial growth of desiring to make nitride-based semiconductor on Sapphire Substrate is to thickness that can self-supporting (Free-standing), then exist since sapphire with the coefficient of thermal expansion differences of nitride-based semiconductor Sapphire Substrate warpage significantly, and then since film thickness increase and the such problem of amount of warpage increase.Therefore, the result cracks in film forming or after the film forming, obtain can self-supporting the nitride-based semiconductor bulk substrate come down to impossible.
As these solution, ELOG (Epitaxial Lateral Over Growth, epitaxial lateral overgrowth) method or DEEP (Dislocation Elimination of Inverted-Pyramidal Pits) method or VAS (Void-Assisted Separation, gap form and peel off) method etc. has been proposed, but, all have the such shortcoming of complex procedures in any one method.
In view of such problem, the objective of the invention is to, nitride semiconductor layer phragmoplast, nitride compound semiconductor device, nitride-based semiconductor bulk substrate and their manufacture method of a kind of Sapphire Substrate and its manufacturing of use are provided, wherein, Sapphire Substrate is the Sapphire Substrate that mainly is used in the epitaxial growth of nitride semiconductor layer, can critically control the warped shapes and/or the amount of warpage of substrate effectively, thereby and the warpage of the substrate that can suppress to produce in the film forming reduce the buckling behavior of substrate.
Present inventors find, inside by the Sapphire Substrate before making the nitride semiconductor layer epitaxial growth, use pulse laser to form the modification area figure, and can control the stress of Sapphire Substrate, thereby can control the warped shapes and/or the amount of warpage of substrate effectively.
In addition, find to use the Sapphire Substrate that obtains by the present invention to form the words of nitride semiconductor layer, can utilize the stress of the Sapphire Substrate that is formed with the modification area figure, the stresses counteract that will produce by film forming, thereby can be suppressed to the warpage of the substrate in the membrane process and reduce the buckling behavior of substrate, thereby finish the present invention.
That is to say, the epitaxial growth of nitride semiconductor layer of the present invention inter-modification Sapphire Substrate, it is employed Sapphire Substrate in the film forming of the nitride semiconductor layer that forms by epitaxial growth, it is characterized in that, inside in above-mentioned Sapphire Substrate, be formed with the modification area figure that has utilized multi-photon to absorb, wherein, the multi-photon absorption is based on pulse laser and produces.
In addition, the epitaxial growth of nitride semiconductor layer of the present invention is characterised in that with the inter-modification Sapphire Substrate, inside in above-mentioned Sapphire Substrate, see through the facet side of above-mentioned Sapphire Substrate and pulse laser is assembled the line scanning of going forward side by side, thereby utilize multi-photon absorb to form the modification area figure and make, wherein, multi-photon absorbs and to be based on pulse laser and to produce.
In addition, the epitaxial growth of nitride semiconductor layer of the present invention is characterised in that with the inter-modification Sapphire Substrate, on the basis of foregoing invention, the flat shape of at least a above-mentioned modification area figure, be banded, latticed, dispose a plurality of polygonal shapes, concentric circles, helical form, be in line symmetry slightly or the slightly point-symmetric shape any one with respect to the straight line of the central point by Sapphire Substrate.
In addition, the epitaxial growth of nitride semiconductor layer of the present invention is characterised in that with the inter-modification Sapphire Substrate, on the basis of foregoing invention, the formation position of at least a above-mentioned modification area figure, it is film forming face from above-mentioned Sapphire Substrate, be the position below 95% more than 3% of substrate thickness, the spacing that constitutes between each line of above-mentioned modification area figure is below the above 2000 μ m of 50 μ m.
In addition, the epitaxial growth of nitride semiconductor layer of the present invention is characterised in that with the inter-modification Sapphire Substrate, on the basis of foregoing invention, the flat shape of at least a above-mentioned modification area figure, be that straight line with respect to the central point by Sapphire Substrate is slightly line symmetry, slightly point-symmetric shape, in latticed any one, the formation position of above-mentioned modification area figure, it is film forming face from Sapphire Substrate, be the position below 50% more than 3% of substrate thickness, the spacing that constitutes between each line of above-mentioned modification area figure is below the above 2000 μ m of 50 μ m.
In addition, nitride semiconductor layer phragmoplast of the present invention is characterised in that, on the film forming face of epitaxial growth with the inter-modification Sapphire Substrate of above-mentioned nitride semiconductor layer, film forming is one deck nitride semiconductor layer and making at least.
In addition, nitride compound semiconductor device of the present invention is characterised in that, uses nitride semiconductor layer phragmoplast of the present invention and makes.
In addition, nitride-based semiconductor bulk substrate of the present invention is characterised in that, uses the thick film of nitride semiconductor layer of the present invention and makes.
In addition, the epitaxial growth of nitride semiconductor layer of the present invention is characterised in that with the inter-modification Sapphire Substrate, using following such modification area figure to form makes with Sapphire Substrate, promptly, the shape of the Sapphire Substrate before above-mentioned modification area figure forms is, the film forming face of above-mentioned semiconductor layer is a concave surface, and the curvature of this concave surface is greater than 0km
-1Smaller or equal to 160km
-1The modification area figure form and to use Sapphire Substrate.
In addition, the epitaxial growth of nitride semiconductor layer of the present invention is characterised in that with the inter-modification Sapphire Substrate, using following such modification area figure to form makes with Sapphire Substrate, promptly, the shape of the Sapphire Substrate before above-mentioned modification area figure forms is, the film forming face of above-mentioned semiconductor layer is a concave surface, and the curvature of this concave surface is 40km
-1Above 150km
-1Following modification area figure forms uses Sapphire Substrate.
In addition, the epitaxial growth of nitride semiconductor layer of the present invention is characterised in that with the inter-modification Sapphire Substrate, using following such modification area figure to form makes with Sapphire Substrate, promptly, the shape of the Sapphire Substrate before above-mentioned modification area figure forms is, the film forming face of above-mentioned semiconductor layer is a concave surface, and the curvature of this concave surface is 85km
-1Above 150km
-1Following modification area figure forms uses Sapphire Substrate.
In addition, modification area figure of the present invention forms and is characterised in that with Sapphire Substrate diameter is below the above 300mm of 50mm, and thickness is below the above 5.0mm of 0.05mm.
Inter-modification Sapphire Substrate of the present invention can be applicable to the epitaxial growth of the various semiconductor layers that comprise nitride-based semiconductor.In addition, can be applicable to the sapphire all single crystals substrate in addition that can utilize pulse laser to form the modification area figure in inside.Particularly, in being used in epitaxially grown single crystalline substrate, owing to be not limited to heteroepitaxial growth, also can solve the problem of the warpage of the substrate that is produced in the isoepitaxial growth that comprises same composition or mix-crystal, be useful therefore.Therefore, can improve the quality or the rate of finished products of various devices or various bulk substrate.
The present invention has following such effect of putting down in writing.
Adopt claim 1 or 2 inventions of being put down in writing, in the single crystalline substrate in the film forming that mainly is used in the crystallinity film that obtains by epitaxial growth, can provide the warped shapes of critically having controlled substrate and/or the single crystalline substrate of amount of warpage effectively.The present invention then is controlled in the difficult heavy caliber substrate of technical change effective especially in the words of only carrying out attrition process.In addition, have the effect that following such single crystalline substrate can be provided, that is, thereby the warpage that can suppress the substrate that produces in the epitaxial growth operation can reduce the single crystalline substrate of the buckling behavior of substrate.
The words of the invention that employing claim 3 is put down in writing, form in the single crystalline substrate of sapphire, nitride-based semiconductor, Si, GaAs, crystal, SiC etc. of modification area figure in substrate interior using pulse laser, have and claim 1 or 2 identical effects.
The invention of adopting claim 4 to put down in writing, because the stresses counteract that can utilize the stress of the single crystalline substrate that is formed with the modification area figure to produce by film forming, therefore, thereby the warpage that can suppress the substrate in the film forming reduces the buckling behavior of substrate.
Consequently, the generation or the non-uniform film thickness homogenize of the dislocation in the crystallinity film can be suppressed, thereby the crystal phragmoplast that the quality of film and uniformity have improved can be accessed.Can use crystal phragmoplast of the present invention to constitute various devices.In addition, crystal phragmoplast of the present invention when forming the thick film with film thickness that can self-supporting by epitaxial growth, can be used as base substrate.
The invention of adopting claim 5 to put down in writing, because the crystal phragmoplast that can use the quality of film and uniformity to improve constitutes various devices, therefore, the various devices that can provide quality and rate of finished products to improve.
The invention of adopting claim 6 to put down in writing owing to can be suppressed in the film forming or the warpage of the substrate that produces after the film forming, therefore, can not used complicated step, in addition the thick film of crystallinity film be grown.Therefore, the various bulk substrate that can provide the thick film by crystallinity film to constitute with film thickness that can self-supporting.
Adopt claim 7 or 8 inventions of being put down in writing, in being used in the epitaxially grown Sapphire Substrate of semiconductor layer, can provide the warped shapes of critically having controlled substrate and/or the Sapphire Substrate of amount of warpage effectively.In addition, adopt Sapphire Substrate of the present invention,, therefore do not need to carry out the cleaning again of substrate owing to be formed with the modification area figure in inside.The present invention then is controlled in the difficult heavy caliber substrate of technical change effective especially in the words of only carrying out attrition process.
In addition, have following such effect, that is, the Sapphire Substrate of the application of the invention can suppress the warpage of the substrate that produces in the epitaxial growth operation of semiconductor layer, thereby can reduce the such effect of buckling behavior of substrate.And then, owing on the Sapphire Substrate surface, do not have figure, therefore, do not need the significantly change of membrance casting condition, thereby can carry out film forming with the condition identical with existing Sapphire Substrate.
The words of the invention that employing claim 9 is put down in writing, because the stresses counteract that can utilize the stress of the Sapphire Substrate that is formed with the modification area figure to produce by the film forming of semiconductor layer, therefore, thus the warpage that can suppress the substrate in the film forming reduces the buckling behavior of substrate.
Consequently, the generation or the non-uniform film thickness homogenize of the dislocation in the semiconductor layer can be suppressed, thereby the semiconductor layer phragmoplast that the quality of film and uniformity have improved can be accessed.Can use semiconductor layer phragmoplast of the present invention to constitute various semiconductor device.In addition, semiconductor layer phragmoplast of the present invention when forming the thick film with film thickness that can self-supporting by epitaxial growth, can be used as base substrate.
The invention of adopting claim 10 to put down in writing, the semiconductor layer phragmoplast that has improved owing to the quality that can use film and uniformity constitutes various semiconductor device, therefore, the various semiconductor device that can provide quality and rate of finished products to improve.
The invention of adopting claim 11 to put down in writing owing to can be suppressed in the film forming of semiconductor layer or the warpage of the substrate that produces after the film forming, therefore, can not used complicated step, not make the thick film growth of semiconductor layer in addition with not cracking.Therefore, the block substrates of various semiconductors that can provide the thick film by semiconductor layer phragmoplast to constitute with film thickness that can self-supporting.
Adopt claim 12 or 13 inventions of being put down in writing, in being used in the epitaxially grown Sapphire Substrate of nitride semiconductor layer, can provide the warped shapes of critically having controlled substrate and/or the Sapphire Substrate of amount of warpage effectively.In addition, adopt Sapphire Substrate of the present invention,, therefore do not need to carry out the cleaning again of substrate owing to be formed with the modification area figure in inside.The present invention then is controlled in the difficult heavy caliber substrate of technical change effective especially in the words of only carrying out attrition process.
In addition, have following such effect, that is, the Sapphire Substrate of the application of the invention can be suppressed at the warpage of the substrate that produces in the epitaxial growth operation of nitride semiconductor layer, thereby can reduce the such effect of buckling behavior of substrate.And then, owing on the surface of Sapphire Substrate, do not have figure, therefore, do not need the significantly change of membrance casting condition, thereby can carry out film forming with the condition identical with existing Sapphire Substrate.
The invention of adopting claim 14 to put down in writing, the effect of record, mainly the warped shapes that can provide substrate also is provided is controlled to the such effect of uniform Sapphire Substrate in claim 12 or 13.
The invention of adopting claim 15 to put down in writing except the effect of record in the claim 12～14, mainly also has the such effect of Sapphire Substrate that the amount of warpage of critically having controlled substrate can be provided.
The words of the invention that employing claim 16 is put down in writing, except the effect of record in the claim 12～14, and then also has an effect that following such Sapphire Substrate can be provided, promptly, the warpage of the substrate that produces in the epitaxial growth operation of nitride semiconductor layer can be suppressed at well, thereby the Sapphire Substrate of the buckling behavior of substrate can be reduced.
The words of the invention that employing claim 17 is put down in writing, because the stresses counteract that can utilize the stress of the Sapphire Substrate that is formed with the modification area figure to produce by the film forming of nitride semiconductor layer, therefore, thus the warpage that can suppress the substrate in the film forming reduces the buckling behavior of substrate.
Consequently, the generation or the non-uniform film thickness homogenize of the dislocation in the nitride semiconductor layer can be suppressed, thereby the nitride semiconductor layer phragmoplast that the quality of film and uniformity have improved can be accessed.Can use nitride semiconductor layer phragmoplast of the present invention and constitute various nitride compound semiconductor devices.In addition, nitride semiconductor layer phragmoplast of the present invention when forming the thick film with film thickness that can self-supporting by epitaxial growth, can be used as base substrate.
The words of the invention that employing claim 18 is put down in writing, the nitride semiconductor layer phragmoplast that has improved owing to the quality that can use film and uniformity constitutes various nitride compound semiconductor devices, therefore, the various nitride compound semiconductor devices that can provide quality and rate of finished products to improve.
The invention of adopting claim 19 to put down in writing as nitride compound semiconductor device, especially can provide in light-emitting component, electronic device, the photo detector any one.
The words of the invention that employing claim 20 is put down in writing, owing to can be suppressed in the film forming of nitride semiconductor layer or the warpage of the substrate that produces after the film forming, therefore, can not use complicated step, the other thick film growth that does not make nitride semiconductor layer with not cracking.Therefore, the various nitride-based semiconductor bulk substrate that can provide the thick film by nitride semiconductor layer phragmoplast to constitute with film thickness that can self-supporting.
The invention of adopting claim 21 to put down in writing as the nitride-based semiconductor bulk substrate, especially can provide by Al
xIn
yGa
zThe nitride-based semiconductor bulk substrate that N (x+y+z=1, x 〉=0, y 〉=0, z 〉=0) constitutes.
The invention of adopting claim 22 to put down in writing can be made the warped shapes of critically having controlled substrate and/or the inter-modification Sapphire Substrate of amount of warpage.
Adopt the words of claim 23 or 24 inventions of being put down in writing, except the effect of record in the claim 22, can also make following such inter-modification Sapphire Substrate, promptly, in the film formation process of underlayer nitriding thing semiconductor layer, thereby the warpage that can suppress substrate reduces the inter-modification Sapphire Substrate of the buckling behavior of substrate.
The words of the invention that employing claim 25 is put down in writing, can make following such inter-modification Sapphire Substrate effectively, promptly, can critically control the warped shapes and/or the amount of warpage of substrate, and in the film formation process of underlayer nitriding thing semiconductor layer, thereby the warpage that can suppress substrate reduces the inter-modification Sapphire Substrate of the buckling behavior of substrate.
The invention of adopting claim 26 to put down in writing can be effectively and critically control the warped shapes and/or the amount of warpage of single crystalline substrate.The present invention then is controlled in the difficult heavy caliber substrate of technical change effective especially in the words of only carrying out attrition process.
The words of the invention that employing claim 27 is put down in writing, form in the single crystalline substrate of sapphire, nitride-based semiconductor, Si, GaAs, crystal, SiC etc. of modification area figure in substrate interior using pulse laser, have the effect identical with claim 26.
The words of the invention that employing claim 28 is put down in writing, thereby owing to can suppress the buckling behavior that the warpage of the substrate in the film forming reduces substrate, therefore, the generation or the non-uniform film thickness homogenize of the dislocation in the crystallinity film can be suppressed, thereby the quality and the uniformity of film can be improved.
The invention of adopting claim 29 to put down in writing, the crystal phragmoplast that has improved owing to the quality that can use film and uniformity constitutes various devices, therefore, can workmanship and the various devices that improved of rate of finished products.
The invention of adopting claim 30 to put down in writing owing to can be suppressed in the film forming or the warpage of the substrate that produces after the film forming, therefore, can not used complicated step, in addition the thick film of crystallinity film be grown.Therefore, can make the various bulk substrate that the thick film by the crystallinity film with film thickness that can self-supporting constitutes.
The invention of adopting claim 31 to put down in writing can be effectively and critically control the warped shapes and/or the amount of warpage of employed Sapphire Substrate in the epitaxial growth of semiconductor layer.The present invention then is controlled in the difficult heavy caliber substrate of technical change effective especially in the words of only carrying out attrition process.In addition, in the present invention owing to be formed with the modification area figure in inside, therefore, have do not need to carry out substrate clean such effect again.
The words of the invention that employing claim 32 is put down in writing, thereby owing to can suppress the buckling behavior that the warpage of the substrate in the film forming reduces substrate, therefore, the generation or the non-uniform film thickness homogenize of the dislocation in the semiconductor layer film forming can be suppressed, thereby the quality and the uniformity of film can be improved.And then have following such effect, that is,, therefore, do not need the significantly change of membrance casting condition, thereby can carry out the such effect of film forming with the condition identical with existing Sapphire Substrate owing on the surface of Sapphire Substrate, do not have figure.
The invention of adopting claim 33 to put down in writing, the semiconductor layer phragmoplast that has improved owing to the quality that can use film and uniformity constitutes various semiconductor device, therefore, can workmanship and the various semiconductor device that improved of rate of finished products.
The invention of adopting claim 34 to put down in writing owing to can be suppressed in the film forming or the warpage of the substrate that produces after the film forming, therefore, can not used complicated step, in addition the thick film of semiconductor layer be grown.Therefore, can make the block substrates of various semiconductors that the thick film by the semiconductor layer with film thickness that can self-supporting constitutes.
The invention of adopting claim 35 to put down in writing can be effectively and critically control the warped shapes and/or the amount of warpage of employed Sapphire Substrate in the epitaxial growth of nitride semiconductor layer.The present invention then is controlled in the difficult heavy caliber substrate of technical change effective especially in the words of only carrying out attrition process.In addition, in the present invention, have owing to form the modification area figure in inside, thus do not need to carry out substrate clean such effect again.
The invention of adopting claim 36 to put down in writing except the effect of record in the claim 35, mainly also has and the warped shapes of Sapphire Substrate can be controlled to evenly such effect.
The invention of adopting claim 37 to put down in writing except the effect of record in the claim 36, mainly also has the such effect of amount of warpage that can critically control Sapphire Substrate.
The words of the invention that employing claim 38 is put down in writing, except the effect of record in the claim 35～37, also have the warpage of the substrate that produces in the epitaxial growth operation that can suppress nitride semiconductor layer more well, thereby reduce the such effect of buckling behavior of Sapphire Substrate.
The words of the invention that employing claim 39 is put down in writing, thereby owing to can suppress the buckling behavior that the warpage of the substrate in the film forming reduces substrate, therefore, the generation or the non-uniform film thickness homogenize of the dislocation in the nitride semiconductor layer film forming can be suppressed, thereby the quality and the uniformity of film can be improved.And then have following such effect, that is,, therefore do not need the significantly change of membrance casting condition, thereby can carry out the such effect of film forming with the condition identical with existing Sapphire Substrate owing on the surface of Sapphire Substrate, do not have figure.
The words of the invention that employing claim 40 is put down in writing, the nitride semiconductor layer phragmoplast that has improved owing to the quality that can use film and uniformity constitutes nitride compound semiconductor device, therefore, can workmanship and the nitride compound semiconductor device that improved of rate of finished products.
The invention of adopting claim 41 to put down in writing as nitride compound semiconductor device, especially can improve any one quality and the rate of finished products in light-emitting component, electronic device, the photo detector.
The invention of adopting claim 42 to put down in writing owing to can be suppressed in the film forming or the warpage of the substrate that produces after the film forming, therefore, can not used complicated step, in addition the thick film of nitride semiconductor layer be grown.Therefore, can make the nitride-based semiconductor bulk substrate that the thick film by the nitride semiconductor layer with film thickness that can self-supporting constitutes.
The invention of adopting claim 43 to put down in writing especially can not made by Al with cracking
xIn
yGa
zThe thick film of the nitride semiconductor layer that N (x+y+z=1, x 〉=0, y 〉=0, z 〉=0) constitutes.
The invention of adopting claim 44 to put down in writing can be made the warped shapes of critically having controlled substrate and/or the inter-modification Sapphire Substrate of amount of warpage effectively.
Adopt the words of claim 45 or 46 inventions of being put down in writing, except the effect of record in the claim 44, can also make following such inter-modification Sapphire Substrate effectively, promptly, in the film formation process of underlayer nitriding thing semiconductor layer, thereby the warpage that can suppress substrate reduces the inter-modification Sapphire Substrate of the buckling behavior of substrate.
The words of the invention that employing claim 47 is put down in writing, can make following such inter-modification Sapphire Substrate effectively, promptly, can critically control the warped shapes and/or the amount of warpage of substrate, and in the film formation process of underlayer nitriding thing semiconductor layer, thereby the warpage that can suppress substrate reduces the inter-modification Sapphire Substrate of the buckling behavior of substrate.
Description of drawings
Fig. 1 is the schematic diagram to single crystalline substrate inside formation modification area that present embodiment relates to.
Fig. 2 is graphics shape, the spacing of the modification area figure that relates to of present embodiment, the schematic diagram of formation position.
Fig. 3 is the schematic diagram of the epitaxial growth operation of the nitride semiconductor layer that relates to of present embodiment.
Fig. 4 is that the In-situ (original position) in the nitride semiconductor growing operation that relates to of present embodiment observes the schematic diagram of example.Wave spectrum A is to use the example of existing Sapphire Substrate, and wave spectrum B, C are to use the example of Sapphire Substrate of the present invention.
Fig. 5 is the schematic diagram of the relation of the amount of warpage of the substrate that relates to of present embodiment and curvature.
Fig. 6 is the use that relates to of present embodiment, and the In-situ of Sapphire Substrate of the present invention (original position) observes the schematic diagram of example.
Fig. 7 is the schematic diagram of dependence of the variable quantity of the substrate curvature after the formation position that relates to of present embodiment 2 and spacing form with respect to the modification area figure.
Fig. 8 a is the schematic diagram of In-situ (original position) observed result of the sample 10 that relates to of present embodiment 3.
Fig. 8 b is the schematic diagram of In-situ (original position) observed result of the sample 12 that relates to of present embodiment 3.
Fig. 8 c is the schematic diagram of In-situ (original position) observed result of the sample 14 that relates to of present embodiment 3.
Fig. 8 d is the schematic diagram of In-situ (original position) observed result of the sample 16 that relates to of present embodiment 3.
Fig. 8 e is the schematic diagram of In-situ (original position) observed result of the sample 18 that relates to of present embodiment 3.
Fig. 8 f is the schematic diagram of In-situ (original position) observed result of the sample 20 that relates to of present embodiment 3.
Embodiment
Below, describe being used to implement suitable mode of the present invention.
Epitaxial growth of the present invention is characterised in that with the inter-modification substrate, the inside of employed single crystalline substrate in the film forming of the crystallinity film that forms by epitaxial growth, see through the facet side of above-mentioned single crystalline substrate and pulse laser is assembled the line scanning of going forward side by side, thereby utilize multi-photon absorb to form the modification area figure and make, wherein, multi-photon absorbs and to be based on above-mentioned pulse laser and to produce.
Single crystalline substrate absorbs and the material that forms modification area in inside gets final product so long as can utilize based on the multi-photon of pulse laser, can enumerate sapphire, nitride-based semiconductor, Si, GaAs, crystal, SiC etc.In addition, also can be quartz or glass etc., rather than single crystalline substrate.
The wavelength of employed pulse laser is suitable than the wavelength in long, the transparent wave band of the absorption edge ripple of the single crystalline substrate that is suitable for.Pulse duration, irradiation energy need be according to the physical characteristics of material and are suitably selected.
In single crystalline substrate is under the situation of Sapphire Substrate, and the wavelength of pulse laser is to be good below the above 5000nm of 200nm, and pulse duration is good with psec～femtosecond, and for better, repetition rate is good with 50kHz～500kHz with 200fs～800fs.Laser power is 0.05～0.8W, and the spot size of laser is 0.5～4 μ m, and spot size is good about with 2 μ m.The sweep speed of sample bench considers that the words of mass productivity are good with 100～1000mm/s.
In addition, the typical processing conditions that can form the modification area in Si, GaAs, the crystal is shown in the table 1.
[table 1]
| Si | GaAs | Quartzy | |
| Wavelength (nm) | 1064 | 1064 | 1045 |
| Pulse duration (sec) | 120×10 -9 | 70×10 -9 | 500×10 -15 |
| Repetition rate (kHz) | 100 | 15 | 100 |
| Spot size (μ m) | 1.5 | 1.5 | 1.0 |
| Laser power (W) | 0.3～1.2 | 0.2 | 0.4 |
| Objective table sweep speed (mm/s) | 200～300 | 200 | 400 |
Under Si, GaAs, quartzy situation, the scope of spot size about with 0.5 μ m～4 μ m is good.The objective table sweep speed is 50mm/s～1000mm/s, considers that the words of mass productivity are good with 100mm/s～1000mm/s.Pulse duration is good with 50ns～200ns under the situation of Si, is good with 30ns～80ns under the situation of GaAs, is good with 200fs～800fs under the situation of crystal.Irradiation energy is respectively being good with 3～12 μ J under the situation of Si, is good with 8～20 μ J under the situation of GaAs, is good with 3～6 μ J under the situation of crystal.Repetition rate is good with 10kHz～500kHz.
The size of single crystalline substrate is not defined, and can use diameter to be the substrate below the above 300mm of 50mm.The thickness of substrate can use the following thickness of the above 5.0mm of 0.05mm.
Single crystalline substrate is as long as the face that is used in the film forming of the crystallinity film that forms by epitaxial growth to the major general grinds.Usually in single crystalline substrate,, and produce warpage because the residual or accurately machined surface roughness of the machining deformation that produces because of grinding is in the top and bottom difference.For example, in the polished substrate of single face, mainly be the main cause that the surface roughness difference of top and bottom becomes warpage, in two-sided polished substrate, except the roughness of top and bottom was slightly different, the surface roughness in substrate surface deviation slightly also became the main cause of warpage.
In addition, so-called " epitaxial growth " comprises the isoepitaxial growth, the heteroepitaxial growth that contain same composition or mix-crystal.
As shown in Figure 1, the facet side that sees through single crystalline substrate 1 is focused at substrate interior with pulse laser 2, and continuously with the high-velocity scanning sample bench, then forms the modification area of the wire that the modification area 3 with point-like couples together continuously.
Part, the modification area 3 of point-like only are formed at by moment ground have been shone on the part of pulse laser, and its size depends on spot size, laser intensity and the pulse duration of laser.In addition, form the distance of modification area 3 of the point-like of wire, form according to the repetition rate of laser and the sweep speed of objective table.
Carry out many combinations by the modification area that these is formed wire, and on the desirable position of the thickness direction of substrate, form at least a modification area figure.So-called " modification area " is multi-photon to take place partly absorb and the metamorphic layer of formation in the part of having shone laser.
As shown in Figure 2, graphics shape by making the modification area figure, the spacing 4 between each line, form the constrained optimization of position 5, modified layer length 6 etc., the stress of substrate integral body can be controlled, thereby the warped shapes and/or the amount of warpage of substrate can be critically controlled.
As graphics shape, for example as shown in Figure 2, its flat shape can form that directional plane (orientation flat) with respect to substrate forms the band shape (Fig. 2 (a) and (b)) of many lines perpendicular or parallelly, latticed (Fig. 2 (c)) etc. of both combinations with this.In addition also can form and dispose a plurality of polygonal shapes (Fig. 2 (d)), concentric circles (Fig. 2 (e)), helical form etc.
Because graphics shape mainly influences the symmetry of the warped shapes of substrate, therefore, desires to obtain uniform warped shapes in substrate surface, its flat shape with the straight line with respect to the central point by substrate serve as slightly the line symmetry or slightly point symmetry such be shaped as good.On the contrary, if flat shape is banded, also may bring deviation to the warped shapes of substrate.
Forming position 5 mainly influences the variable quantity of the amount of warpage of the substrate after the modification area figure forms, and then variable quantity is big more the closer to the surface to form the position.For the film forming face to single crystalline substrate is not brought influence, the formation position of at least a modification area figure, with the film forming face with substrate be set in as benchmark more than 3% below 95% of substrate thickness, suitable more be to be good below 50% 3% or more.Also a plurality of modification area figures can be formed on the different formation position of thickness direction of substrate.
Modified layer length 6 forms according to spot size, irradiation energy (laser power/repetition rate), the pulse duration of laser, forms to count the thickness about μ m～tens of μ m usually.
As mentioned above, by at the inner stress that forms the modification area figure and control substrate of single crystalline substrate, can obtain the warped shapes of substrate and/or the inter-modification substrate that amount of warpage is critically controlled effectively.
In addition, on the film forming face of the inter-modification substrate that obtains by the present invention, form one deck crystallinity film at least by epitaxial growth, thereby can make the crystal phragmoplast.The formation method of crystallinity film can be suitable for any one of vapor phase growth, liquid growth.For example, can use various crystal growths such as MBE method (molecular beam epitaxy), CVD method (chemical vapour deposition technique), VPE method (vapour phase epitaxy method), LPE method (liquid phase epitaxial method), sublimed method.
Use inter-modification substrate of the present invention, because the stresses counteract that can utilize the stress of inter-modification substrate to produce by film forming, therefore, thereby the warpage that can suppress the substrate in the film forming reduces the buckling behavior of substrate.Therefore, can the be improved quality and the inhomogeneity crystal phragmoplast of crystallinity film.
Use constitutes various devices by the crystal phragmoplast that the present invention obtains, and can improve the quality and the rate of finished products of device.
In addition, crystal phragmoplast of the present invention can be used as base material, and then be formed the thick film of crystallinity film by isoepitaxial growth with film thickness that can self-supporting (Free-standing).In addition, the base material separation of thick film from being made of the crystal phragmoplast with the crystallinity film can access bulk substrate (bulk substrate).
And then, by thick film and the modification substrate separation internally that on inter-modification substrate of the present invention, forms the crystallinity film, also can access the bulk substrate that the thick film by the crystallinity film constitutes.Use inter-modification substrate of the present invention,, therefore, can not form thick film with cracking owing to can be suppressed in the film forming or the warpage of the substrate that produces after the film forming.
As film thickness that can self-supporting, being good more than the 50 μ m.In addition, as the formation method of thick film, can use mocvd method (Metalorganic chemical vapor deposition method), HVPE method (hydride vapour phase epitaxy method), LPE method (liquid phase epitaxial method) etc.
By using Sapphire Substrate as above-mentioned single crystalline substrate, can access the inter-modification Sapphire Substrate, wherein, this inter-modification Sapphire Substrate has the effect identical with above-mentioned inter-modification substrate, and, be suitable for the film forming of the semiconductor layer that forms by epitaxial growth.
In addition, on the film forming face of inter-modification Sapphire Substrate of the present invention, form one semiconductor layer at least, thereby can make the semiconductor layer phragmoplast by epitaxial growth.Can access semiconductor device and the block substrate of semiconductor that semiconductor layer phragmoplast that use obtains by the present invention constitutes.
Particularly, be under the situation of nitride semiconductor layer at semiconductor layer, employed Sapphire Substrate in the film forming as nitride semiconductor layer can use diameter to be the substrate below the above 300mm of 50mm.The present invention is owing to have bigger effect in the heavy caliber substrate, therefore, be more than the 75mm and then particularly useful in the substrate greater than 150mm at diameter.Substrate dimension and above-mentioned irrelevant and unqualified.
The thickness of employed Sapphire Substrate in the film forming of nitride semiconductor layer can adopt the following thickness of the above 5.0mm of 0.05mm.For the modification area figure being formed on the position of not destroying Sapphire Substrate itself, the thickness of substrate is being good more than the 0.1mm.In addition, suitable more is, the diameter of substrate be under the situation below the above 150mm of 50mm with 0.3mm more than for good, more than the diameter of substrate surpasses under the situation of 150mm with 0.5mm, be good.
In addition, can use the film forming face of nitride semiconductor layer to be concave surface, and the curvature of this concave surface is greater than 0km
-1Smaller or equal to 160km
-1Substrate.
When the inside of employed Sapphire Substrate forms the modification area figure in the film forming of nitride semiconductor layer, the flat shape of figure, as described above be banded, latticed, dispose a plurality of polygonal shapes, concentric circles, helical form, with respect to the straight line of the central point by substrate be line symmetry slightly or slightly any one in the such shape of point symmetry for good.In order to obtain in substrate surface, having the inter-modification Sapphire Substrate of uniform warped shapes and amount of warpage, being that straight line with respect to the central point by substrate is line symmetry slightly, slightly point-symmetric shape, in latticed any one is shaped as better.
Spacing between each line is good with 50 μ m～2000 μ m, with 100 μ m～1000 μ m for better.And then consider mass productivity, with 200 μ m～500 μ m for better.
The formation position of at least a modification area figure, with the film forming face with substrate be set at as benchmark be formed at substrate thickness more than 3% below 95% for good, suitable more is more than 3% below 50%.Also a plurality of modification area figures can be formed on the different formation position of thickness direction of substrate.
In addition, under the prior art, when the light-emitting component that the Sapphire Substrate upper strata is pressed with nitride semiconductor layer is cut apart, after the film forming of nitride semiconductor layer with Sapphire Substrate brilliant back-grinding processing (back-grinding) to 100 μ m after, at the inner figure of cutting apart usefulness that forms of Sapphire Substrate, but, also the flat shape of the modification area figure that is provided with before the film forming of nitride semiconductor layer can be formed latticed, and finally as led chip cut apart with and use.Under this situation, being formed at figure, to stay on the position such in the remaining thickness part in brilliant back-grinding processing back of Sapphire Substrate be desirable.
Below, on the film forming face of the inter-modification Sapphire Substrate that obtains by the present invention, make one deck nitride semiconductor layer epitaxial growth at least and the mode of making the nitride semiconductor layer phragmoplast is narrated.
In Fig. 3 (a)～(d), represent epitaxial growth operation to the nitride semiconductor layer that carries out on the Sapphire Substrate.On film build method, can use mocvd method, HVPE method, MBE method etc.At first, carry out the heat of Sapphire Substrate 7 and clean (thermal cleaning) (Fig. 3 (a)), and carry out the growth (Fig. 3 (b)) of low temperature buffer layer 8.Then, the InGaN that make n-GaN layer 9 (Fig. 3 (c)), has a multi-quantum pit structure (Multiple quantum well structures) is active layer 10 (Fig. 3 (d)) growth.
In-situ (original position) in Fig. 4 in the epitaxial growth operation of expression nitride semiconductor layer observes example.As disclosed in the non-patent literature 2, can analyze the behavior of the Sapphire Substrate in the film forming quantitatively by In-situ (original position) observation.That is to say, can know that the warped shapes of substrate or amount of warpage are in film forming as where change.
In Fig. 4, transverse axis is the time, and the longitudinal axis is expressed as the curvature (km of the substrate of face
-1).It is convex-shaped that the forward of the longitudinal axis is expressed as face, and it is concave shape that negative sense is expressed as face.
Can calculate the amount of warpage of substrate by the flexometer of substrate.That is to say, as shown in Figure 5, if the radius of curvature of substrate is made as R, then has the amount of warpage X (μ m) of the substrate of 1/R curvature, use as D approx by diameter substrate, can be simply be as 0.322 * curvature (km under the situation of 50mm at the diameter of substrate
-1) and obtain, be as 1.250 * curvature (km at the diameter of substrate under the situation of 150mm
-1) and obtain.
Wave spectrum A among Fig. 4, the example of the existing Sapphire Substrate that does not form the modification area figure is used in expression.
In addition, Fig. 4 (a)～(e) is corresponding with each process of film formation process respectively.That is to say, (a) clean corresponding to the heat of substrate, (b) corresponding to the low temperature buffer layer growth, (c) corresponding to the n-GaN layer growth, is the active layer growth corresponding to InGaN (d), (e) corresponding to cooling.
Use the wave spectrum A of Fig. 4, the behavior of the substrate among Fig. 4 (a)～(e) is described.
Cleaning in the stage of transition to (a) substrate heat, and since the temperature difference on the top and bottom of Sapphire Substrate, the further grow of the concave of substrate aufwuchsplate, thus curvature significantly changes.
Then, usually temperature is being reduced to about 500～600 ℃ and in the stage of (b) low temperature buffer layer growth transition, the concave of substrate weakens, thereby curvature diminish a little.
Then, once more temperature is increased to about 1000 ℃ and carries out in the stage of (c) n-GaN layer growth, because gallium nitride is poor with sapphire lattice constant, and make the concave grow of substrate, thereby curvature becomes greatly.And then carry out film forming, because the big more then curvature of film thickness is big more, therefore, the remarkable variation of substrate inner evenness of film thickness and film quality.Only controlling by membrance casting condition that the substrate inner evenness is considered to is difficult technically.In addition, in nitride semiconductor layer, thereby the situation that produces dislocation film quality variation in order to relax stress becomes problem.
Then, temperature is reduced to about 700～800 ℃, at (d) InGaN is in the growth phase of active layer, influences the inner evenness of emission wavelength because InGaN is the film thickness of active layer and the uniformity of the composition of the In among the InGaN, thereby influences the fabrication yield of led chip.Influenced by film-forming temperature because InGaN is the film thickness or the In composition of active layer, therefore, in order to improve the temperature homogeneity in the substrate surface, making the curvature of the substrate in the film forming is desirable near 0 as much as possible.
At last, in the stage of (e) cooling substrate, because once more because of coefficient of thermal expansion differences makes substrate shape warpage significantly once more, therefore, the curvature of the substrate after a series of film formation process finishes becomes big.This causes producing makes the preceding brilliant back-grinding processing of led chipization become the such problem of difficulty.
More than, by shown in the wave spectrum A of Fig. 4 as can be known, use the words of existing Sapphire Substrate, can make InGaN is that substrate curvature in the active layer growth phase is almost 0, on the other hand, exist the behavior of the substrate in the film formation process big, the curvature of the substrate after film forming finishes becomes big such shortcoming.
Next, first example that will observe by the In-situ (original position) when the inner formation of existing Sapphire Substrate modification area figure is made inter-modification Sapphire Substrate of the present invention and film forming nitride semiconductor layer is shown in the wave spectrum B among Fig. 4.
The initial condition of the inter-modification Sapphire Substrate among the wave spectrum B is that to form the modification area figure like that be good to convex surface to compare the film forming face warpage with existing Sapphire Substrate.By like this, compare with the wave spectrum A that uses existing Sapphire Substrate, can reduce the buckling behavior of substrate.
Among the wave spectrum C in Fig. 4, similarly represented to use the example of inter-modification Sapphire Substrate with the situation of wave spectrum B, wherein, this inter-modification Sapphire Substrate, be when the inner formation of existing Sapphire Substrate modification area figure, adjust spacing between each line and figure and form the position, the initial condition that makes Sapphire Substrate compare wave spectrum B and further significantly warpage be the inter-modification Sapphire Substrate of convex surface.
Wave spectrum C can further reduce the behavior of substrate by film formation process.That is to say that the stress that produces in the stresses counteract film forming of utilizing substrate is compared in expression with wave spectrum A, B effect is bigger.
Compare with the situation of using existing Sapphire Substrate, with above-mentioned wave spectrum B, the nitride semiconductor layer that C obtains, because the warpage of the substrate in the film forming is suppressed, the buckling behavior of substrate diminishes, so the quality of film and uniformity raising.
But simultaneously, the initial condition of inter-modification Sapphire Substrate is significantly, and warpage is the state of convex surface, the result is, the curvature of the substrate when producing InGaN and be the active layer growth phase and finishing with film forming is compared with the situation of using existing Sapphire Substrate and become such problem greatly.
That is to say, inter-modification Sapphire Substrate of the present invention, shown in the wave spectrum C among Fig. 6, forming can be when reducing the buckling behavior of substrate, and making InGaN is that the curvature of active layer growth phase and the film forming substrate when finishing such initial condition that diminishes is desirable.
By like this, can improve the uniformity of the emission wavelength of nitride semiconductor luminescent element in the quality and the inhomogeneity while of the film that improves nitride semiconductor layer.
Therefore, in the Sapphire Substrate before the modification area figure forms, use can be in advance with by the formation of modification area figure significantly warpage be desirable as the such Sapphire Substrate of the substrate curvature partial offset of convex surface.
As mentioned above, as the Sapphire Substrate of modification area figure formation usefulness, can use the film forming face of nitride semiconductor layer to be concave surface, and the curvature of this concave surface is greater than 0km
-1Smaller or equal to 160km
-1Sapphire Substrate.In addition, from above-mentioned reason, be concave surface with the film forming face of nitride semiconductor layer, and the curvature of this concave surface is 40km
-1Above 150km
-1Below be good, and then with 85km
-1Above 150km
-1Below for better.
As mentioned above, the inter-modification Sapphire Substrate of the application of the invention can access the nitride semiconductor layer phragmoplast that the quality of film of nitride semiconductor layer and uniformity have improved.
Use nitride semiconductor layer phragmoplast of the present invention, can constitute the nitride compound semiconductor device of light-emitting component that quality and rate of finished products improved, electronic device, photo detector etc.
In addition, on nitride semiconductor layer phragmoplast of the present invention, and then form by epitaxial growth after the thick film of nitride semiconductor layer with film thickness that can self-supporting, the above-mentioned nitride semiconductor layer phragmoplast that to use as base substrate is separated, and can access the nitride-based semiconductor bulk substrate that the thick film by nitride semiconductor layer constitutes.
In addition, on inter-modification Sapphire Substrate of the present invention, form the words of the thick film of above-mentioned nitride semiconductor layer, can be suppressed in the film forming or the warpage of the substrate that produces after the film forming, thereby can obtain having the thick film of the nitride semiconductor layer of film thickness that can self-supporting with not cracking.Thick film by the nitride semiconductor layer that will obtain like this is from above-mentioned inter-modification substrate separation, can not use complicated step and obtains the nitride-based semiconductor bulk substrate.As the nitride-based semiconductor bulk substrate, especially can make by Al effectively
xIn
yGa
zThe nitride-based semiconductor bulk substrate that N (x+y+z=1, x 〉=0, y 〉=0, z 〉=0) constitutes.
Embodiment
Next, the embodiment that the present invention relates to is described particularly.Use the lasing condition shown in the table 2 to form the modification area figure in that Sapphire Substrate is inner, and investigated influence for the variation of the warped shapes of substrate and amount of warpage.Its result is shown in embodiment 1 and 2.
[table 2]
| Wavelength (nm) | 1045 |
| Pulse duration (sec) | 500×10 -15 |
| Repetition rate (kHz) | 100 |
| Spot size (μ m) | 1.6～3.5μm |
| Laser power (W) | 0.3 |
| Objective table sweep speed (mm/s) | 400 |
(embodiment 1)
As the Sapphire Substrate that forms the modification area figure, use the polished 2 inches Sapphire Substrate of single face.Substrate thickness is 430 μ m.The warped shapes and the amount of warpage of the substrate before the modification area figure forms utilize laser interferometer to measure.
Then, Sapphire Substrate is arranged on the sample bench of impulse laser unit, has carried out formation the modification area figure of Sapphire Substrate inside.
The graphics shape of sample 1～9, spacing, formation position and the modified layer length between each line, the machining schedule of each piece are shown in Table 3.The substrate shape of the Sapphire Substrate after the modification area figure forms utilizes laser interferometer to measure, and amount of warpage and substrate thickness utilize linear measurement meter and laser interferometer to measure.In table 3, ⊥ O.F. represents vertical with the directional plane of Sapphire Substrate, //O.F. represents parallel with directional plane.
[table 3]
The symmetry of the warped shapes in the substrate surface after warped shapes, amount of warpage and the figure of the substrate before and after the modification area figure formed forms is shown in the table 4.The warped shapes of substrate is expressed as the shape of face side.
[table 4]
(embodiment 2)
As the Sapphire Substrate that forms the inter-modification regional graphics, use the polished 4 inches Sapphire Substrate of single face.Substrate thickness is 650 μ m.The warped shapes and the amount of warpage of the substrate before similarly to Example 1, the modification area figure forms utilize laser interferometer to measure.
Then, Sapphire Substrate is arranged on the sample bench of impulse laser unit, has carried out formation the modification area figure of Sapphire Substrate inside.Graphics shape, spacing, the formation position of sample 10～19 are shown in the table 5.
[table 5]
The warped shapes of the substrate after the modification area figure forms utilizes laser interferometer to measure, and amount of warpage utilizes the linear measurement meter to measure.Substrate shape before and after the modification area figure formed, amount of warpage and compare and be shown in the table 6 by the curvature that amount of warpage calculates.The warped shapes of substrate is expressed as the shape of face side.
[table 6]
In addition, the dependence with the variable quantity of the substrate curvature after forming spacing between position and each line and forming with respect to the modification area figure is shown among Fig. 7.
(embodiment 3)
To in embodiment 2, form the sample 10,12,14,16,18 in the Sapphire Substrate of modification area figure, the existing Sapphire Substrate (as sample 20) that does not form figure imports in the MOCVD device simultaneously, and has carried out the growth to the gallium nitride layer on the Sapphire Substrate.Growth temperature and film thickness in each film forming engineering are shown in the table 7.
[table 7]
| Growth temperature (℃) | Film thickness (nm) | |
| The AlGaN resilient coating | 550 | 500 |
| The n-GaN layer | 1070 | 5000 |
| The GaN/InGaN active layer | 750 | 100/2 |
In-situ (original position) observed result of each sample is shown among Fig. 8 a～Fig. 8 f, warped shapes, amount of warpage and the curvature of the substrate of each sample is shown in the table 8, the variable quantity of the substrate curvature in each stage is shown in the table 9.
(1) in the table 9～(4), illustrated among Fig. 8 a, when expression (1) is cleaned transition with respect to the heat of substrate initial condition respectively, during GaN/InGaN active layer growth transition during with respect to the n-GaN growth ending of (2) during with respect to the n-GaN layer growth of substrate initial condition, (3),
(4) variable quantity of the curvature after finishing with respect to the cooling of substrate initial condition.
[table 8]
[table 9]
The variable quantity of the substrate curvature when (1) is cleaned transition by substrate initial condition thermotropism in sample 10,12,14,16,18 that has formed the inter-modification regional graphics and the sample 20 that do not form figure, is not found the big poor of curvature changing amount.
Variable quantity from (2) substrate curvature during with respect to the n-GaN layer growth of substrate initial condition, figure is being formed in the more shallow locational sample 10,16,18 in Sapphire Substrate surface, is comparing the effect of the variable quantity inhibition of the substrate curvature when having found n-GaN grown with other sample.
The variable quantity of the substrate curvature during from (3) GaN/InGaN active layer growth transition during with respect to the n-GaN growth ending, when the n-GaN layer growth finishes to the stage of GaN/InGaN active layer growth transition, figure being formed in the more shallow locational sample 10,16,18 in Sapphire Substrate surface, compare the effect of having found the variable quantity inhibition of substrate curvature with other sample.
The variable quantity of the substrate curvature after finishing with respect to the cooling of substrate initial condition from (4), figure being formed in the more shallow locational sample 10,16,18 in Sapphire Substrate surface, compare the effect of having found the variable quantity inhibition of substrate curvature with other sample.
Film thickness uniformity and crystal mass to the gallium nitride layer of the sample 10,12,14,16,18,20 that obtains by above operation are investigated.
The sample 20 of learning and not forming the modification area figure is compared, and the film thickness uniformity of sample 10 improves.Think that this is because by figure being formed on more shallow position, Sapphire Substrate surface, and carry out the n-GaN layer growth with the more smooth state of substrate shape.
And then, measure (001) face of the gallium nitride layer that (X-ray diffraction rocking curve measurements) obtain, FWHM (full width at half maximum (FWHM)) value of (102) face by the X-ray diffraction swing curve, in sample 10, be respectively 203arcsec, 418arcsec, in the sample 20 that does not form the modification area figure, be respectively 242arcsec, 579arcsec.The result in the sample 10 that has formed the modification area figure, compares with the sample 20 that does not form the modification area figure as can be known thus, and the crystallinity of gallium nitride layer improves.
By above result as can be known, use inter-modification Sapphire Substrate of the present invention to carry out the epitaxially grown words of nitride semiconductor layer, owing to the warpage that can suppress substrate reduces the buckling behavior of substrate, so the quality of film and uniformity improve.
Symbol description
1 single crystalline substrate
2 pulse lasers
3 modification areas
4 spacings
5 form the position
6 modified layer length
7 Sapphire Substrate
8 low temperature buffer layers
The 9n-GaN layer
10InGaN is an active layer
Claims (47)
1. epitaxial growth inter-modification substrate is an employed single crystalline substrate in the film forming of the crystallinity film that forms by epitaxial growth, it is characterized in that,
In the inside of described single crystalline substrate, be formed with the modification area figure that has utilized multi-photon to absorb, wherein, the multi-photon absorption is based on pulse laser and produces.
2. epitaxial growth inter-modification substrate is an employed single crystalline substrate in the film forming of the crystallinity film that forms by epitaxial growth, it is characterized in that,
Inside in described single crystalline substrate, see through the facet side of described single crystalline substrate and pulse laser is assembled the line scanning of going forward side by side, thereby utilize multi-photon to absorb and form the modification area figure and manufactured, wherein, the multi-photon absorption is based on described pulse laser and produces.
3. epitaxial growth inter-modification substrate as claimed in claim 1 or 2 is characterized in that the material of described single crystalline substrate is any one among sapphire, nitride-based semiconductor, Si, GaAs, crystal, the SiC.
4. a crystal phragmoplast is characterized in that, on the film forming face of any epitaxial growth of being put down in writing with the inter-modification substrate of claim 1～3, film forming has one deck crystallinity film at least.
5. a device is characterized in that, is provided with the crystal phragmoplast that claim 4 is put down in writing.
6. a bulk substrate is characterized in that, the thick film of the crystallinity film of being put down in writing by claim 4 constitutes.
7. semiconductor layer epitaxial growth inter-modification Sapphire Substrate is an employed Sapphire Substrate in the film forming of the semiconductor layer that forms by epitaxial growth, it is characterized in that,
In the inside of described Sapphire Substrate, be formed with the modification area figure that has utilized multi-photon to absorb, wherein, the multi-photon absorption is based on pulse laser and produces.
8. epitaxial growth inter-modification Sapphire Substrate is an employed Sapphire Substrate in the film forming of the semiconductor layer that forms by epitaxial growth, it is characterized in that,
Inside in described Sapphire Substrate, see through the facet side of described Sapphire Substrate and pulse laser is assembled the line scanning of going forward side by side, thereby utilize multi-photon to absorb and form the modification area figure and manufactured, wherein, the multi-photon absorption is based on described pulse laser and produces.
9. a semiconductor layer phragmoplast is characterized in that, on the film forming face of semiconductor layer epitaxial growth with the inter-modification Sapphire Substrate that claim 7 or 8 is put down in writing, film forming has one semiconductor layer at least.
10. a semiconductor device is characterized in that, is provided with the semiconductor layer phragmoplast that claim 9 is put down in writing.
11. the block substrate of a semiconductor is characterized in that, the thick film of the semiconductor layer of being put down in writing by claim 9 constitutes.
12. the epitaxial growth of nitride semiconductor layer inter-modification Sapphire Substrate is an employed Sapphire Substrate in the film forming of the nitride semiconductor layer that forms by epitaxial growth, it is characterized in that,
In the inside of described Sapphire Substrate, be formed with the modification area figure that has utilized multi-photon to absorb, wherein, the multi-photon absorption is based on pulse laser and produces.
13. the epitaxial growth of nitride semiconductor layer inter-modification Sapphire Substrate is an employed Sapphire Substrate in the film forming of the nitride semiconductor layer that forms by epitaxial growth, it is characterized in that,
Inside in described Sapphire Substrate, see through the facet side of described Sapphire Substrate and pulse laser is assembled the line scanning of going forward side by side, thereby utilize multi-photon to absorb and form the modification area figure and manufactured, wherein, the multi-photon absorption is based on described pulse laser and produces.
14. the epitaxial growth inter-modification Sapphire Substrate as claim 12 or 13 described nitride semiconductor layers is characterized in that,
The flat shape of at least a described modification area figure, for banded, latticed, dispose a plurality of polygonal shapes, concentric circles, helical form, be in line symmetry slightly or the slightly point-symmetric shape any one with respect to the straight line of the central point by Sapphire Substrate.
15. the epitaxial growth inter-modification Sapphire Substrate as any described nitride semiconductor layer of claim 14 is characterized in that,
The formation position of at least a described modification area figure is the film forming face from described Sapphire Substrate, is the position below 95% more than 3% of substrate thickness,
The spacing that constitutes between each line of described modification area figure is below the above 2000 μ m of 50 μ m.
16. the epitaxial growth inter-modification Sapphire Substrate as any described nitride semiconductor layer of claim 14 is characterized in that,
The flat shape of at least a described modification area figure, for the straight line with respect to the central point by Sapphire Substrate is line symmetry slightly, slightly point-symmetric shape, in latticed any one,
The formation position of described modification area figure is the film forming face from Sapphire Substrate, is the position below 50% more than 3% of substrate thickness,
The spacing that constitutes between each line of described modification area figure is below the above 2000 μ m of 50 μ m.
17. a nitride semiconductor layer phragmoplast is characterized in that, on the film forming face of epitaxial growth with the inter-modification Sapphire Substrate of the nitride semiconductor layer that claim 12～16 is put down in writing, film forming has one deck nitride semiconductor layer at least.
18. a nitride compound semiconductor device is characterized in that, is provided with the nitride semiconductor layer phragmoplast that claim 17 is put down in writing.
19. nitride compound semiconductor device as claimed in claim 18 is characterized in that, described nitride compound semiconductor device is any one in light-emitting component, electronic device, the photo detector.
20. a nitride-based semiconductor bulk substrate is characterized in that, the thick film of the nitride semiconductor layer of being put down in writing by claim 17 constitutes.
21. nitride-based semiconductor bulk substrate as claimed in claim 20 is characterized in that, described nitride-based semiconductor bulk substrate is by Al
xIn
yGa
zN (x+y+z=1, x 〉=0, y 〉=0, z 〉=0) constitutes.
Use Sapphire Substrate 22. a modification area figure forms, it is characterized in that, in claim 7～21, the shape of the Sapphire Substrate before described modification area figure forms is that the film forming face of described semiconductor layer is a concave surface, and the curvature of this concave surface is greater than 0km
-1Smaller or equal to 160km
-1
Use Sapphire Substrate 23. a modification area figure forms, it is characterized in that, in claim 7～21, the shape of the Sapphire Substrate before described modification area figure forms is that the film forming face of described semiconductor layer is a concave surface, and the curvature of this concave surface is 40km
-1Above 150km
-1Below.
Use Sapphire Substrate 24. a modification area figure forms, it is characterized in that, in claim 7～21, the shape of the Sapphire Substrate before described modification area figure forms is that the film forming face of described semiconductor layer is a concave surface, and the curvature of this concave surface is 85km
-1Above 150km
-1Below.
25. any described modification area figure formation Sapphire Substrate as claim 22～24, it is characterized in that, the diameter of the Sapphire Substrate before described modification area figure forms is below the above 300mm of 50mm, and thickness is below the above 5.0mm of 0.05mm.
26. the epitaxial growth manufacture method of inter-modification substrate is characterized in that,
The inside of employed single crystalline substrate in the film forming of the crystallinity film that forms by epitaxial growth, see through the facet side of described single crystalline substrate and pulse laser is assembled the line scanning of going forward side by side, form the modification area figure thereby utilize multi-photon to absorb, and control the warped shapes and/or the amount of warpage of described single crystalline substrate, wherein, multi-photon absorbs and to be based on described pulse laser and to produce.
27. the epitaxial growth as claimed in claim 26 manufacture method of inter-modification substrate is characterized in that,
The material of described single crystalline substrate is any one among sapphire, nitride-based semiconductor, Si, GaAs, crystal, the SiC.
28. the manufacture method of a crystal phragmoplast is characterized in that, on the film forming face of epitaxial growth with the inter-modification substrate that claim 26 or 27 is put down in writing, film forming is one deck crystallinity film at least.
29. the manufacture method of a device is characterized in that, uses the crystal phragmoplast that claim 28 puts down in writing and makes.
30. the manufacture method of a bulk substrate is characterized in that, uses the thick film of the crystal phragmoplast that claim 28 puts down in writing and makes.
31. the semiconductor layer epitaxial growth manufacture method of inter-modification substrate is characterized in that,
The inside of employed Sapphire Substrate in the film forming of the semiconductor layer that forms by epitaxial growth, see through the facet side of described Sapphire Substrate and pulse laser is assembled the line scanning of going forward side by side, form the modification area figure thereby utilize multi-photon to absorb, and control the warped shapes and/or the amount of warpage of described single crystalline substrate, wherein, multi-photon absorbs and to be based on described pulse laser and to produce.
32. the manufacture method of a semiconductor layer phragmoplast is characterized in that, on the film forming face of semiconductor layer epitaxial growth with the inter-modification Sapphire Substrate that claim 31 is put down in writing, forms one semiconductor layer at least.
33. the manufacture method of a semiconductor device is characterized in that, uses the semiconductor layer phragmoplast of being put down in writing in the claim 32 and makes.
34. the manufacture method of the block substrate of a semiconductor is characterized in that, uses the thick film of the semiconductor layer phragmoplast of being put down in writing in the claim 32 and makes.
35. the epitaxial growth of the nitride semiconductor layer manufacture method of inter-modification substrate is characterized in that,
The inside of employed Sapphire Substrate in the film forming of the nitride semiconductor layer that forms by epitaxial growth, see through the facet side of described Sapphire Substrate and pulse laser is assembled the line scanning of going forward side by side, form the modification area figure thereby utilize multi-photon to absorb, and control the warped shapes and/or the amount of warpage of described single crystalline substrate, wherein, multi-photon absorbs and to be based on described pulse laser and to produce.
36. the epitaxial growth of the nitride semiconductor layer as claimed in claim 35 manufacture method of inter-modification Sapphire Substrate is characterized in that,
The flat shape of at least a described modification area figure, for banded, latticed, dispose a plurality of polygonal shapes, concentric circles, helical form, be in line symmetry slightly or the slightly point-symmetric shape any one with respect to the straight line of the central point by Sapphire Substrate.
37. the epitaxial growth of the nitride semiconductor layer as claimed in claim 36 manufacture method of inter-modification Sapphire Substrate is characterized in that,
The formation position of at least a described modification area figure is the film forming face from described Sapphire Substrate, is the position below 95% more than 3% of substrate thickness,
The spacing that constitutes between each line of described modification area figure is below the above 2000 μ m of 50 μ m.
38. the epitaxial growth of the nitride semiconductor layer as claimed in claim 36 manufacture method of inter-modification Sapphire Substrate is characterized in that,
The flat shape of at least a described modification area figure is that the straight line with respect to the central point by Sapphire Substrate is slightly line symmetry, slightly point-symmetric shape or latticed,
The formation position of described modification area figure is the film forming face from Sapphire Substrate, is the position below 50% more than 3% of substrate thickness,
The spacing that constitutes between each line of described modification area figure is below the above 2000 μ m of 50 μ m.
39. the manufacture method of a nitride semiconductor layer phragmoplast is characterized in that, on the film forming face of epitaxial growth with the inter-modification Sapphire Substrate of the nitride semiconductor layer that claim 35～38 is put down in writing, forms one deck nitride semiconductor layer at least.
40. the manufacture method of a nitride compound semiconductor device is characterized in that, uses the nitride semiconductor layer phragmoplast of being put down in writing in the claim 39 and makes.
41. the manufacture method of nitride compound semiconductor device as claimed in claim 40 is characterized in that, described nitride compound semiconductor device is any one in light-emitting component, electronic device, the photo detector.
42. the manufacture method of a nitride-based semiconductor bulk substrate is characterized in that, uses the thick film of the nitride semiconductor layer phragmoplast of being put down in writing in the claim 39 and makes.
43. nitride-based semiconductor bulk substrate as claimed in claim 42 is characterized in that, described nitride-based semiconductor bulk substrate is by Al
xIn
yGa
zN (x+y+z=1, x 〉=0, y 〉=0, z 〉=0) constitutes.
44. the semiconductor layer epitaxial growth manufacture method of inter-modification Sapphire Substrate is characterized in that,
In claim 31～43, the shape of the Sapphire Substrate before described modification area figure forms is that the film forming face of described semiconductor layer is a concave surface, and the inverse of the curvature of this concave surface is greater than 0km
-1Smaller or equal to 160km
-1
45. the semiconductor layer epitaxial growth manufacture method of inter-modification Sapphire Substrate is characterized in that,
In claim 31～43, the shape of the Sapphire Substrate before described modification area figure forms is that the film forming face of described semiconductor layer is a concave surface, and the inverse of the curvature of this concave surface is 40km
-1Above 150km
-1Below.
46. the semiconductor layer epitaxial growth manufacture method of inter-modification Sapphire Substrate is characterized in that,
In claim 31～43, the shape of the Sapphire Substrate before described modification area figure forms is that the film forming face of described semiconductor layer is a concave surface, and the inverse of the curvature of this concave surface is 85km
-1Above 150km
-1Below.
47. the semiconductor layer epitaxial growth manufacture method of inter-modification Sapphire Substrate is characterized in that,
In claim 44～46, the diameter of the Sapphire Substrate before described modification area figure forms is below the above 300mm of 50mm, and thickness is below the above 5.0mm of 0.05mm.
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| JP2009-006293 | 2009-01-15 | ||
| JP2009006293A JP5552627B2 (en) | 2009-01-15 | 2009-01-15 | Internally modified substrate for epitaxial growth, crystal film formed by using the same, device, bulk substrate, and manufacturing method thereof |
| PCT/JP2009/006633 WO2010082267A1 (en) | 2009-01-15 | 2009-12-04 | Inside reforming substrate for epitaxial growth; crystal film forming element, device, and bulk substrate produced using the same; and method for producing the same |
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Also Published As
| Publication number | Publication date |
|---|---|
| TWI494476B (en) | 2015-08-01 |
| TW201033413A (en) | 2010-09-16 |
| KR101362859B1 (en) | 2014-02-17 |
| US20120018732A1 (en) | 2012-01-26 |
| KR20110129377A (en) | 2011-12-01 |
| JP5552627B2 (en) | 2014-07-16 |
| CN102272891B (en) | 2015-06-17 |
| EP2388802A4 (en) | 2013-03-06 |
| EP2388802A1 (en) | 2011-11-23 |
| PL2388802T3 (en) | 2016-02-29 |
| WO2010082267A1 (en) | 2010-07-22 |
| JP2010165817A (en) | 2010-07-29 |
| EP2388802B1 (en) | 2015-05-06 |
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